•  
  •  
  •  
  •  
  •  
  •  
  •  
  •  
期刊检索


检索
检索项:
检索词:
总目录
  • WCSB9︱2019(第九届)世界采样和混样大会 查看全文>>
  • 关于召开第十五届全国青年分析测试学术报告会的通知 查看全文>>
友情链接
双水相萃取/超高效液相色谱-串联质谱法测定倒提壶中8种生物碱
    点此下载全文
作者单位
樊轻亚,许卫军,代春美 1.信阳职业技术学院药学院
2.中国中医科学院 
基金项目:河南省科技厅科技攻关项目(172102310315);第24批博士后科技服务团合作项目
中文摘要:建立了乙醇-磷酸氢二钾双水相萃取技术结合超高效液相色谱-串联质谱法(UHPLC-MS/MS)同时测定倒提壶中8种生物碱含量的方法。采用单因素实验考察了双水相的萃取条件对倒提壶中8种生物碱萃取率的影响,最佳萃取条件为:乙醇质量分数为30%,K2HPO4·3H2O的质量分数为20%,萃取剂与样品相比为6∶1,水相的pH值为4.0。以乙腈-0.1 mol/L醋酸铵为流动相进行UHPLC-MS/MS分析,8种生物碱之间具有良好的分离度,各成分在一定质量浓度范围内具有良好的线性关系(r2>0.99)。方法的精密度、重复性及加标回收率的相对标准偏差(RSD)均小于 3.0%。方法简单快捷、灵敏准确,可满足倒提壶中生物碱检测的要求。
中文关键词:倒提壶  生物碱  双水相萃取  超高效液相色谱-串联质谱法(UHPLC-MS/MS)
 
Determination of Eight Alkaloids in Cynoglossum amabile Stapf et Drumm by Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry with Aqueous Two phase Extraction
Abstract:An ultrahigh performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS) with EtOH/K2HPO4·3H2O aqueous two-phase extraction was developed for the simultaneous determination of eight alkaloids in Cynoglossum amabile Stapf et Drumm.Effects of aqueous two phase extraction conditions on extraction efficiencies of eight alkaloids were optimized by single factor experiment.The optimum conditions were as follows:30%(mass ratio) of ethanol,20%(mass ratio) of K2HPO4·3H2O,6∶1 for an extractant to sample ratio,and 4.0 for pH value.The extract was analyzed by UHPLC-MS/MS with acetonitrile-0.1 mol/L ammonium acetate as mobile phases,and eight alkaloids in the extract were well separated.There were good linear relationships for the analytes in the certain concentration ranges with their correlation coefficients(r2) larger than 0.99.The relative standard deviations(RSDs) for precision,reproducibility and recovery were all less than 3.0%.The method is convenient,sensitive and accurate,and is suitable for the determination and confirmation of eight alkaloids in Cynoglossum amabile Stapf et Drumm.
Key Words:Cynoglossum amabile Stapf et Drumm  alkaloid  aqueous two phase extraction  ultra high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)
引用本文:樊轻亚,许卫军,代春美.双水相萃取/超高效液相色谱-串联质谱法测定倒提壶中8种生物碱[J].分析测试学报,2019,38(11):1328-1334.
摘要点击次数: 122
全文下载次数: 109
查看全文  查看/发表评论  下载PDF阅读器